Olive cotton-dye and process of making same.



UNITED STATES PATENT OFFICE.

ERNST GOEBEL, OF ELBERFELD, GERMANY, ASSIGNOR TO THE FARBEN- FABRIKEN OFELBERFELD COMPANY, OF NEW YORK.

OLIVE COTTON-DYE AND PROCESS OF MAKING SAME.

SPECIFICATION forming part of Letters Patent N 0. 653,670, dated July17, 1900.

Application filed October 31, 1899. Serial No. 735,409- (Specimens) ToaZZ whom it rnrty concern.-

Be it known that I, ERNST GOEBEL, doctor of philosophy, chemist,residing at Elberfeld, Germany, (assignor to the FARBENFABRIKEN OFELBERFELD COMPANY, of New York,) have invented a new and usefulImprovement in Olive Cotton-Dye; and I hereby declare the following tobe a clear and exact description of my invention.

I have found that valuable coloring-matters dyeing unmordanted cottonfrom greenish-olive to olive and brownish-olive shades are obtained ifcertain methylized derivatives of amidodinitrodiphenylamin having theformula (R meaning a hydrogen atom which may be replaced by a methylicgroup) are subjected at elevated temperatures to the action of alkalinesulfid-carrying compounds, such as mixtures of sodium or potassiumsultid and sulfur, sulfur and soda, sulfur and potassa, sodiumpolysulfid, potassium polysulfid, or the like. The dyestufis thusobtained are dark powders, which are soluble in water by a ten-per-cent.ammonia liquor. They are dissolved with an olive color. As abovementioned, they dye unmordanted cotton in hot baths containing sodiumsulfid and common salt from greenish-olive to olive and brownish-oliveshades.

It may be remarked that the bodies which are used as bases or startingmaterials in the present process can be easily produced by the action ofl 3 at dinitrochlorobenzeue 0n monomethylized orunsymmetrically-d1methylized diamins of the general formula NH O H, OH

(R meaning in this formula a hydrogen atom which may be replaced by amethylic group,) such as paraamidomonomethylanilin,paraamidodimethylanilin, metaamidodimethylanilin,orthoamidodimethylanilin, or the like.

In order to illustrate my new process more fully, the following exampleis given, the parts being by weight: To a mixture prepared from eightyparts of dry sodium sulfid, sixty parts of sulfur, and thirty parts ofwater, which mixture is heated in an iron vessel provided with astirring apparatus, forty parts of dimethylamidodinitrodiphenylaminhaving the formula (which can be obtained by the action of 1 3 4dinitrochlorobenzene on paraamidodimethylanilin, (see Berz'chte derDeutschen Chemischen Gesellschafl, Vol. XXIII, p. 2739) are added withstirring at about from to centigrade. The temperature is then slowlyraised to about from to cent-igrade, the mass being stirred the while.When the whole mass becomes solid, the iron vessel is closed and thetemperature of the mixture is by and by raised to from 280 to 290centigrade. The melt is kept at this temperature until the quantity ofthe dyestuff formed during the reaction no longer increases.Subsequently the melt is allowed to cool. When cool it represents a darksolid mass which can easily be pulverized and directly be used for dyein which formula-R means a hydrogen atom which may be replaced by amethylic group, and secondly heating the resulting mixture at elevatedtemperatures, substantially as hereinbefore described.

2. The process for producing a new dyestuff, which process consists infirst mixing at about from 90 to 100 centigrade an alkalinesulfid-carrying compound with dimethylparaamidodinitrodiphenylamin ofthe formula:

and secondly heating the resulting mixture at elevated temperatures,substantially as hereinbefore described.

3. As new articles of manufacture the new dyestuffs obtained frommethylized derivatives of amidodinitrodiphen ylamin of the gen, eralformula which dyestuffs are dark powders soluble in water, beingdissolved by a ten-per-cent. ammonia liquor with an olive color, dyeingunmordanted cotton in hot baths containing sodium sulfid and common saltfrom greenisholive, to olive and brownish-olive shades, substantially ashereinbefore described.

4. As a new article of manufacture the new rdyestuff obtained fromdimethylparaamido- 'dinitrodiphenylamin of the formula being a darkpowder, soluble in water with a yellowish-olive color, in a dilutesodium-sulfid solution, a dilute sodium-carbonate solution and in aten-per-cent. ammonia liquor with an olive color, being dissolved by adilute soda-lye with a green color, dyeing unmordanted cotton in hotbaths containing sodium sulfid and common salt intense and fast oliveshades substantially as hereinbefore described.

In testimony whereof I have signed my name in the presence of twosubscribing witnesses.

ERNST GOEBEL.

Witnesses:

R. E. JAHN, OTTO Rome.

It is hereby certified that in Letters Patent No. 653,670, granted July17, 1900, upon the application of Ernst Goebel, of Elberfeld, Germany,for an improvement in Olive Cotton-Dyes and Processes of Making Same, anerror appears in the printed specification requiring correction, asfollows: In line 14, page 2, the Word amido dinitrophenylamin shouldread amidedinitrodiphenylamin; and that the said Letters Patent shouldbe read with this correction therein that the same may conform to therecord of the case in the Patent Oifice.

Signed, countersigned, and sealed this 7th day of August, A. D., 1900.

F. L. CAMPBELL, Assistant Secretary of the Interim,

[SEAL] Countersigned WALTER H. OHAMBERLIN,

Acting Commissioner of Patents.

